SUPERCRITICAL FLUID EXTRACTION OF ACORUS CALAMUS L. ANALYSIS BY GAS CHROMATOGRAPHY- MASS SPECTROMETRY
Simion Gocan1, Simona Cobzac1, Eda Prodan1, Vladimir Ciovarnache2
1 Universitatea Babeş-Bolyai,Facultatea de Chimie şi Inginerie Chimica,Cluj-Napoca,
2I.C.P.T. Câmpina, Prahova
Essential oils of Acorus calamus L. (A. calamus) are highly complex mixtures. In the earlier papers were reported that the essential oil of the root of A. calamus is composed of a-pinen, champhen, champhor, borneol, and sequiterpene [1], reducing sugars, tannins, resins, sterol, and 1,5% essential oil [2]. The A.calamus L. essential oil obtained by steam distillation from rhizome of the Romanian plant was investigated by GC-MS [3,4].
The present paper reports on the replacement of steam distillation or alcoholic extraction with supercritical fluid extraction (SFE). A total af 27 major components were detected, only 12 e.g. asarone, shyobunone and acorenone were identified on the basis of their MS spectra, by comparison with the spectra library (Wiley and NIST).
Table 1.
The composition of Acorus Calamus L. extract obtained through supercritical fluid extraction and analyzed by GC-MS
No / Compound / Molecular ion (m/z) / tR (min) / Concentration (%)1
2
3
4
5
6
7
8
9
10
11
12 / Methyl eugenol Benzene,1,2-dimetoxy-4-(1-propenil)
Benzene,1-(1,5-dimethyl-4-hexenyl)-4-methyl Criptoacorone
a-Selinene
Preisocalamendiol
Asarone
Benzene,1,2,4-trimetoxy-5-(1-propenil) Calamenol
Shyobunone, Isoshyobunone, Epishyobynone
(+)-3,8-Dimethyl-5-(1-methyllethylidene)-1,2,3,4,5,6,7,8-octahidroazulene-6-one
Calacone 1,4-Trans-1,7-trans-acorenone
Calamendiol
Isoacorone
Acorone / 178
202
208
204
220
208
193
220
218
220
236
218 / 12.98
13.56
14.05
14.16
14.31
14.53
15.36
15.73
16.23
16.63
18.39
18.61 / 0.46
0.12
2.12
0.48
4.48
10.40
1.91
18.31
6.20
16.23
1.24
2.10
The results shows considerable qualitative and quantitative differences between the extract compozition obtained in supercritical conditions, volatile fraction of an alcoholic extract [5] and an essential oil obtained by steam distillation [6]. The supercritical fluid extraction with CO2 has provided a sample with a great number of extracted compounds.
Reference
1. G.P.Pivnenko, R.K.Chargovets, O.V.Chaiko, M.F.Loknvitskaya, T.Khar’Kov, The chemical and antibacterial properties of the essential oil of Accorus root,Farmatsevt. Inst.1957, No.1 294-299;Refrat. Zuhr.Khim., Biol.Khim., 1958, Abstr. No. 27435; C.A.,53(1959), 4425a.
2. B.C.Bose, R.Vijayvargirja, A.Q.Saifi, S.K.Sharma, Chemical and PharmacologicalStudies of Acorus calamus, J.Am.Pharm.Assoc., Sci.Ed., 49(1960), 32-34.
3. R.Oprean, M.Tamas, R.Sandulescu, L.Roman, Essential oils analysis. I. Evaluation of essential oils composition using both GC and MS fingerprints, J.Pharm.Biomed.Anal., 18(1998), 651-657.
4. R.Oprean, L.Oprean, M.Tamas, R.Sandulescu, L.Roman, Essential oils. II. Mass spectra identification of terpene and phenilpropane derivatives, J.Pharm.Biomed.Anal., 24(2001), 1163-1168.
5. 19 G.Mazza, Gas chromatographic and mass spectrometric studies of the constituents of the rhizome of Calamus, J.Chromatogr., 328(1985), 179-194
6. G.Mazza, Gas chromatographic and mass spectrometric studies of the constituents of the rhizome of Calamus, J.Chromatogr., 328(1985), 195-206.